Anguizola Jeanethe, Bi Cong, Koke Michelle, Jackson Abby, Hage David S
Chemistry Department, University of Nebraska, 704 Hamilton Hall, Lincoln, NE, 68588, USA.
Anal Bioanal Chem. 2016 Aug;408(21):5745-5756. doi: 10.1007/s00216-016-9677-7. Epub 2016 Jun 11.
An on-column approach for protein entrapment was developed to immobilize alpha1-acid glycoprotein (AGP) for drug-protein binding studies based on high-performance affinity chromatography. Soluble AGP was physically entrapped by using microcolumns that contained hydrazide-activated porous silica and by employing mildly oxidized glycogen as a capping agent. Three on-column entrapment methods were evaluated and compared to a previous slurry-based entrapment method. The final selected method was used to prepare 1.0 cm × 2.1 mm I.D. affinity microcolumns that contained up to 21 (±4) μg AGP and that could be used over the course of more than 150 sample applications. Frontal analysis and zonal elution studies were performed on these affinity microcolumns to examine the binding of various drugs with the entrapped AGP. Site-selective competition studies were also conducted for these drugs. The results showed good agreement with previous observations for these drug-protein systems and with binding constants that have been reported in the literature. The entrapment method developed in this study should be useful for future work in the area of personalized medicine and in the high-throughput screening of drug interactions with AGP or other proteins. Graphical abstract On-column protein entrapment using a hydrazide-activated support and oxidized glycogen as a capping agent.
基于高效亲和色谱法,开发了一种柱上蛋白质截留方法,用于固定α1-酸性糖蛋白(AGP)以进行药物-蛋白质结合研究。通过使用含有酰肼活化多孔硅胶的微柱,并采用轻度氧化的糖原作为封端剂,将可溶性AGP物理截留。评估了三种柱上截留方法,并与之前的基于浆料的截留方法进行了比较。最终选择的方法用于制备内径为1.0 cm×2.1 mm的亲和微柱,该微柱含有高达21(±4)μg的AGP,可在超过150次样品应用过程中使用。对这些亲和微柱进行了前沿分析和区域洗脱研究,以检查各种药物与截留的AGP的结合情况。还对这些药物进行了位点选择性竞争研究。结果与之前对这些药物-蛋白质系统的观察结果以及文献中报道的结合常数显示出良好的一致性。本研究中开发的截留方法应有助于个性化医疗领域以及AGP或其他蛋白质与药物相互作用的高通量筛选的未来工作。图形摘要 使用酰肼活化载体和氧化糖原作为封端剂的柱上蛋白质截留。